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Sodium Carbonate → 3-(2-Chloro-5-nitrophenyl)pyridine

HRID 586303
ノート
印刷プレビュー

反応式

HRID 586303 の反応式
Br[C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8].B1([C:18]2[CH:23]=[CH:22][CH:21]=[N:20][CH:19]=2)OCCCO1.C([O-])([O-])=O.[Na+].[Na+]>C(O)C.C1(C)C=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Cl:8][C:7]1[CH:6]=[CH:5][C:4]([N+:9]([O-:11])=[O:10])=[CH:3][C:2]=1[C:18]1[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 10340Sodium CarbonateHCID 27355492-Bromo-1-chloro-4-nitrobenzeneHCID 41980053-(1,3,2-Dioxaborinan-2-yl)pyridine

生成物 1

HCID 223295393-(2-Chloro-5-nitrophenyl)pyridine収率 69%

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒
HCID 702
Ethanol
溶媒
HCID 1140Toluene溶媒

実験手順

A mixture of 3-bromo-4-chloronitrobenzene (5.17 g, 21.9 mmol) and pyridine-3-boronic acid 1,3-propanediol cyclic ester (4.27 g, 26.2 mmol) in ethanol (30 ml) and toluene (30 ml) together with 2 N Na2CO3 solution (13.9 ml) was degassed with a stream of nitrogen for 10 min. Tetrakis(triphenylphosphine)palladium(0) (0.3 g, 0.26 mmol) was added and the reaction was heated at reflux for over 24 h. The mixture was concentrated under reduced pressure to remove the organic solvents and water (100 ml) was added. This was extracted with ethyl acetate (200 ml) and then washed with brine (75 ml), dried (MgSO4), and concentrated under reduced pressure while dry loading onto silica. The resulting crude residue was purified by column chromatography (silica gel, 50% Et2O/CH2Cl2), to yield the title compound (3.53 g, 69%): 1H NMR (360 MHz, CDCl3) δ 7.42-7.48 (1H, m), 7.70 (1H, d, J 8.7 Hz), 7.81 (1H, dt, J 8.0, 1.8 Hz), 8.17-8.27 (2H, m), 8.68-8.77 (2H, m).

後処理

  1. customwas degassed with a stream of nitrogen for 10 min
  2. temperaturethe reaction was heated
  3. temperatureat reflux for over 24 h
  4. concentrationThe mixture was concentrated under reduced pressure
  5. customto remove the organic solvents and water (100 ml)
  6. additionwas added
  7. extractionThis was extracted with ethyl acetate (200 ml)
  8. washwashed with brine (75 ml)
  9. dry with materialdried (MgSO4)
  10. concentrationconcentrated under reduced pressure
  11. customwhile dry loading onto silica
  12. customThe resulting crude residue was purified by column chromatography (silica gel, 50% Et2O/CH2Cl2)

出典と根拠

ORDレコード
ord-5d81ba80b27c4c67a0b4b11fdd25b41e
出典データセット
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06936608B2

反応ノート

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